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CIQTEK EPR200M with 3D-Printed Electrolytic Cell Enables Operando Detection of Radical Intermediates
CIQTEK EPR200M with 3D-Printed Electrolytic Cell Enables Operando Detection of Radical Intermediates
Understanding the formation of radical intermediates is key to controlling electrochemical reaction rates and selectivity. These short-lived species at the electrode interface dictate outcomes, and relying solely on final products can lead to speculative mechanisms. With operando EPR using CIQTEK benchtop EPR200M, researchers can directly capture radicals in situ, mapping their formation sequence and structural fingerprints for robust mechanistic evidence. A recent collaboration between Beijing University of Technology (Sun Zaicheng / Liu Yichang), Tsinghua University (Yang Haijun), and Wuhan University (Lei Aiwen) introduced a novel 3D-printed electrolytic cell tailored for in situ EPR. Fabricated with high-precision digital light processing (DLP), this flat cell enables reproducible integration with electrochemical systems. Their results, published in Chemical Engineering Journal under the title Bespoke electrolytic cell for operando EPR tests: Revealing the formation and accurate structures of amino and phenolic radicals, demonstrate the workflow’s ability to uncover radical structures across representative reactions.   Methodological Breakthrough: 3D-Printed Flat Electrolytic Cell for Reproducible Operando EPR High-dielectric solvents commonly used in electrochemical cells reduce EPR signal-to-noise, making radical detection challenging. The flat cell design mitigates dielectric losses and enhances the resonator’s Q factor, improving operando EPR performance. Beyond physics, the cell is engineered for reproducibility. Using DLP 3D printing, electrode channels, positioning structures, and short-circuit protection are fixed during fabrication. This eliminates manual variability, reduces system resistance, and improves signal quality, while maintaining mechanical strength, solvent compatibility, and cost efficiency. This approach transforms operando EPR into a workflow of "standardized structural component + reproducible procedure", enabling cross-team and cross-system reproducibility and mechanistic comparison.   Time-Resolved Evidence Tracks Radical Formation in C–N Coupling In situ EPR with time-resolved acquisition allows mapping radicals in real-time, showing which species appear first and how they evolve. This provides a reproducible evidence chain at the intermediate level, moving mechanistic understanding beyond product-based inference.   Cycloaddition Intermediates Reveal Reaction Selectivity By comparing substrate-specific spectra and calculating spin density, EPR signals are directly translated into radical structural fingerprints. This forms a closed-loop framework for explaining regio- and chemo-selectivity in (3+2) cycloaddition reactions.   Solvent Effects Guide C–O Coupling Design In situ EPR shows that the same radical exhibits distinct spectra in MeCN versus HFIP. Combined with NMR, the study links solvent, radical structure, and reaction selectivity, providing an experimental evidenc...
CIQTEK SNVM Reveals Magnon Transport in BiFeO₃ (Advanced Functional Materials)
CIQTEK SNVM Reveals Magnon Transport in BiFeO₃ (Advanced Functional Materials)
With the support of CIQTEK Scanning NV Microscopy (SNVM), researchers at Tsinghua University have directly visualized nanoscale spin cycloid structures in multiferroic BiFeO₃. This work, published in Advanced Functional Materials, provides the missing microscopic evidence linking crystal symmetry, magnetic structure, and anisotropic magnon transport, highlighting SNVM as a decisive tool for magnonics and low-power spintronic research.   The study used the CIQTEK Scanning NV Probe Microscope (SNVM) Research Background: Magnon Transport in Multiferroic Oxides Magnon-mediated spin currents can propagate in magnetically ordered insulators with nearly zero energy dissipation, making them highly attractive for next-generation low-power spintronic devices. In multiferroic materials such as BiFeO₃, the coupling between ferroelectric and antiferromagnetic orders enables electric field control of magnons, a long-standing goal in spintronics. Despite this promise, the microscopic origin of weakly anisotropic magnon transport in rhombohedral phase BiFeO₃, commonly referred to as R-BFO, has remained unresolved. Addressing this challenge requires direct real-space characterization of nanoscale magnetic structures, which has long been inaccessible using conventional techniques.   Technical Bottleneck: Lack of Direct Magnetic Structure Evidence Theoretical studies have predicted that R-BFO hosts a cycloidal spin structure that plays a critical role in suppressing strong anisotropy in magnon transport. However, experimental confirmation has been elusive. Traditional characterization techniques, such as X-ray magnetic linear dichroism, provide spatially averaged magnetic information and are unable to resolve nanoscale spin textures. As a result, the logical connection between crystal symmetry, magnetic structure, and magnon transport remained incomplete due to the absence of direct microscopic magnetic imaging.   CIQTEK SNVM Approach: Direct Nanoscale Magnetic Imaging CIQTEK Scanning NV Microscopy (SNVM) overcomes these limitations by combining nanometer-scale spatial resolution with electron spin level magnetic field sensitivity. This enables non-invasive, quantitative imaging of local magnetic fields generated by complex spin textures inside functional materials. In this work, the research teams led by Prof. Yi Di from the State Key Laboratory of New Ceramic Materials and Prof. Nan Tianxiang from the School of Integrated Circuits at Tsinghua University employed CIQTEK SNVM magnetic imaging to directly probe the intrinsic magnetic structure of R-BFO.   Key Findings Enabled by SNVM Magnetic Imaging Using CIQTEK SNVM, the researchers clearly observed a uniform cycloidal spin structure within R-BFO, with a characteristic periodicity of approximately 70 nanometers. The high spatial resolution of SNVM allowed precise quantification of the cycloid wavelength and confirmed that the magnetic structure exists in a single-domain state. By correlating SN...
Corrosion Science Spotlight: CIQTEK SEM in Steam Oxide Film Analysis
Corrosion Science Spotlight: CIQTEK SEM in Steam Oxide Film Analysis
Nuclear fusion is considered a key future energy source due to its high efficiency and clean energy output. In fusion reactors, water cooling systems are widely used because they are technically mature, cost-effective, and have excellent cooling performance. However, a major challenge remains: under high temperature and high pressure, water and steam strongly corrode structural materials. While this problem has been studied in fission reactors, fusion environments are more complex. The unique high-intensity, unevenly distributed magnetic fields in fusion devices interact with corrosion processes, creating new technical challenges that need detailed research. To address this, Associate Professor Peng Lei's team from the University of Science and Technology of China conducted an in-depth study using the CIQTEK scanning electron microscope (SEM) and dual-beam electron microscope. They built high-temperature magnetic-field steam corrosion and high-temperature water corrosion setups. Using SEM, EBSD, and FIB techniques, they analyzed oxide films formed on CLF-1 steel after 0–300 hours of steam corrosion at 400°C under 0T, 0.28T, and 0.46T magnetic fields, and after 1000 hours of high-temperature water corrosion at 300°C.   The study used CIQTEK SEM5000X ultra-high-resolution field-emission SEM and the FIB-SEM DB500   The study found that the oxide films form a multilayer structure, with a chromium-rich inner layer and an iron-rich outer layer. Film formation occurs in five stages: initial oxide particles, then floc-like structures, formation of a dense layer, growth of spinel structures on the dense layer, and finally, spinel cracking into laminated oxides. The presence of a magnetic field significantly accelerates corrosion, promotes the transformation of outer magnetite (Fe₃O₄) into hematite (Fe₂O₃), and enhances laminated oxide formation. This work was published in Corrosion Science, a top-tier journal in the field of corrosion and materials degradation, under the title: "Magnetic field effects on the high-temperature steam corrosion behavior of reduced activation ferritic/martensitic steel."     Surface Oxide Film Characterization In high-temperature steam (HTS), CLF-1 steel surfaces show different corrosion states over time. On polished surfaces, early-stage oxidation (60 h) appears as small, dispersed particles. The Fe/Cr ratio is similar to the substrate, indicating that the oxide layer is not yet complete. By 120 h, floc-like oxides appear. At 200 h, a dense oxide layer forms, with new oxide particles and local spinel structures on top. Rough surfaces corrode faster. Early floc-like oxides are finer and more evenly distributed. By 200 h, they transform into spinel structures, showing a stronger difference from polished surfaces. In high-temperature, high-pressure water (HTPW), polished surfaces display similar spinel structures. Spinel in HTPW is denser and more numerous, while spinel in HTS is larger in size....
CIQTEK SEM and EPR Reveal a New Pathway for Nickel-Citrate Removal
CIQTEK SEM and EPR Reveal a New Pathway for Nickel-Citrate Removal
With the rapid expansion of new energy, mining, metallurgy, and electroplating industries, nickel pollution in water bodies has become a growing threat to environmental quality and human health. During industrial processes, nickel ions often interact with various chemical additives to form highly stable heavy-metal organic complexes (HMCs). In nickel electroplating, for example, citrate (Cit) is widely used to improve coating uniformity and brightness, but the two carboxyl groups in Cit readily coordinate with Ni²⁺ to form Ni–Citrate (Ni-Cit) complexes (logβ = 6.86). These complexes significantly alter nickel’s charge, steric configuration, mobility, and ecological risks, while their stability makes them challenging to remove with conventional precipitation or adsorption methods. Currently, "complex dissociation" is regarded as the key step in removing HMCs. However, typical oxidation or chemical treatments suffer from high cost and complicated operation. Therefore, multifunctional materials with both oxidative and adsorptive capabilities offer a promising alternative. Researchers from Beihang University, led by Prof. Xiaomin Li and Prof. Wenhong Fan, used the CIQTEK scanning electron microscope (SEM) and electron paramagnetic resonance (EPR) spectrometer to conduct an in-depth investigation. They developed a new strategy using KOH-modified Arundo donax L. biochar to efficiently remove Ni-Cit from water. The modified biochar not only showed high removal efficiency but also enabled nickel recovery on the biochar surface. The study, titled “Removal of Nickel-Citrate by KOH-Modified Arundo donax L. Biochar: Critical Role of Persistent Free Radicals”, was recently published in Water Research.     Material Characterization Biochar was produced from Arundo donax leaves and impregnated with KOH at different mass ratios. SEM imaging (Fig. 1) revealed: The original biochar (BC) exhibited a disordered rod-like morphology. At a 1:1 KOH-to-biomass ratio (1KBC), an ordered honeycomb-like porous structure was formed. At ratios of 0.5:1 or 1.5:1, pores were underdeveloped or collapsed. BET analysis confirmed the highest surface area for 1KBC (574.2 m²/g), far exceeding other samples. SEM and BET characterization provided clear evidence that KOH modification dramatically enhances porosity and surface area—key factors for adsorption and redox reactivity.   Figure 1. Preparation and characterization of KOH-modified biochar.   Performance in Ni-Cit Removal Figure 2. (a) Removal efficiency of total Ni by different biochars; (b) TOC variation during Ni–Cit treatment; (c) Effect of Ni–Cit concentration on the removal efficiency of 1KBC; (d) Effect of pH on the removal performance of 1KBC; (e) Influence of coexisting ions on Ni–Cit removal by 1KBC; (f) Continuous-flow removal performance of Ni–Cit by 1KBC. (Ni–Cit = 50 mg/L, biochar dosage = 1 g/L)   Batch experiments de...
CIQTEK SEM Study Shows Raised-Ring Electrodes Improve Aluminum Alloy Spot Welding and Electrode Life
CIQTEK SEM Study Shows Raised-Ring Electrodes Improve Aluminum Alloy Spot Welding and Electrode Life
Aluminum alloys, prized for their exceptional strength-to-weight ratio, are ideal materials for automotive lightweighting. Resistance spot welding (RSW) remains the mainstream joining method for automotive body manufacturing. However, the high thermal and electrical conductivity of aluminum, combined with its surface oxide layer, requires welding currents far exceeding those used for steel. This accelerates copper electrode wear, leading to unstable weld quality, frequent electrode maintenance, and increased production costs. Extending electrode life while ensuring weld quality has become a critical technological bottleneck in the industry.   To address this challenge, Dr. Yang Shanglu's team at Shanghai Institute of Optics and Fine Mechanics conducted an in-depth study using the CIQTEK FESEM SEM5000. They innovatively designed a raised-ring electrode and systematically investigated the effect of ring number (0–4) on electrode morphology, revealing the intrinsic relationship between ring count, crystal defects in the weld nugget, and current distribution. Their results show that increasing the number of raised rings optimizes current distribution, improves thermal input efficiency, enlarges the weld nugget, and significantly extends electrode lifespan. Notably, the raised rings enhance oxide layer penetration, improving current flow while reducing pitting corrosion. This innovative electrode design provides a new technical approach for mitigating electrode wear and lays a theoretical and practical foundation for broader application of aluminum alloy RSW in the automotive industry. The study is published in the Journal of Materials Processing Tech. under the title “Investigating the Influence of Electrode Surface Morphology on Aluminum Alloy Resistance Spot Welding.” Raised-Ring Electrode Design Breakthrough Facing the electrode wear challenge, the team approached the problem from electrode morphology. They machined 0 to 4 concentric raised rings on the end face of conventional spherical electrodes, forming a novel Newton Ring electrode (NTR).   Figure 1. Surface morphology and cross-sectional profile of the electrodes used in the experiment   SEM Analysis Reveals Crystal Defects and Performance Enhancement How do raised rings influence welding performance? Using the CIQTEK FESEM SEM5000 and EBSD techniques, the team characterized the microstructure of weld nuggets in detail. They found that the raised rings pierce the aluminum oxide layer during welding, optimizing current distribution, influencing heat input, and promoting nugget growth. More importantly, the mechanical interaction between raised rings and molten metal significantly increases the density of crystal defects, such as geometrically necessary dislocations (GNDs) and low-angle grain boundaries (LAGBs), within the weld nugget. Optimal performance was observed with three raised rings (NTR3).   Figure 2. EBSD analysis of weld nugget microstruct...
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